CN116875958B - Cr 5 Te 8 Electromagnetic wave-absorbing material of @ expanded graphite and preparation method and application thereof - Google Patents
Cr 5 Te 8 Electromagnetic wave-absorbing material of @ expanded graphite and preparation method and application thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000011358 absorbing material Substances 0.000 title claims abstract description 49
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 46
- 239000010439 graphite Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 5
- 238000005516 engineering process Methods 0.000 claims abstract description 5
- 239000010453 quartz Substances 0.000 claims description 49
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 49
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 42
- 238000010438 heat treatment Methods 0.000 claims description 33
- 229910052786 argon Inorganic materials 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 14
- 239000012159 carrier gas Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 238000011144 upstream manufacturing Methods 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 230000007480 spreading Effects 0.000 claims description 2
- 238000003892 spreading Methods 0.000 claims description 2
- 239000011651 chromium Substances 0.000 claims 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 230000010287 polarization Effects 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 3
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- 238000010924 continuous production Methods 0.000 abstract 1
- 102000020897 Formins Human genes 0.000 description 11
- 108091022623 Formins Proteins 0.000 description 11
- 238000011068 loading method Methods 0.000 description 9
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- 238000004088 simulation Methods 0.000 description 5
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 229910005900 GeTe Inorganic materials 0.000 description 1
- 239000002800 charge carrier Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
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- 230000004044 response Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
- -1 transition metal chalcogenides Chemical class 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
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Abstract
The invention provides Cr 5 Te 8 An electromagnetic wave-absorbing material of expanded graphite, a preparation method and application thereof, belonging to the technical field of electromagnetic wave-absorbing materials; in the method, a one-step chemical vapor deposition technology is utilized to construct two-dimensional Cr 5 Te 8 Cr with heterostructure under synergistic action of atomic spin magnetism and light porous conductive expanded graphite magnetoelectricity of nanosheets 5 Te 8 An expanded graphite wave-absorbing material; cr (Cr) 5 Te 8 Intimate contact with the expanded graphite may trigger the redistribution of interfacial charges, thereby producing a secondary Cr 5 Te 8 The built-in electric field and the Schottky barrier to the expanded graphite are beneficial to the dense polarization of the interface and the electromagnetic energy consumption. The preparation method is simple, convenient and efficient, has low production cost, is suitable for industrial amplified continuous production, and is expected to be widely applied to the fields of electromagnetic protection of electronic equipment, stealth materials and the like.
Description
Technical Field
The invention belongs to the technical field of electromagnetic wave-absorbing materials, and relates to Cr 5 Te 8 An electromagnetic wave-absorbing material of expanded graphite, a preparation method and application thereof.
Background
With the increasing complexity of the application environment of electromagnetic stealth materials, there is an urgent need to explore new wave absorbing materials to address challenges. In recent years, two-dimensional (2D) materials represented by various materials such as graphene, mxnes, transition metal chalcogenides (TMDs, transition Metal Dichalcogenides) and the like are being used in applications in the fields of electronic communication security, electromagnetic protection and the like, with their excellent properties and various varieties.
Notably, TMDs (V, cr, mn, fe, cd, pt and Pd based) provide a unique platform for exploring new electromagnetic protection materials, benefiting from their unique properties: (i) The two-dimensional layered structure provides rich electromagnetic scattering sites for TMDs-based wave absorbing materials, and when electromagnetic waves penetrate into the network, excited electrons can migrate along the axial direction or other adjacent lamellae; (ii) The strong spin orbit coupling and valley polarization of the charge carriers are automatically converted into spin polarization, so that the dissipation of electromagnetic waves on the atomic level is improved; (iii) Various electronic band structures including materials such as conductors, semi-metals, semiconductors, insulators, and superconductors; TMDs are made ideal traders for heterogeneous interface engineering, which can increase the consumption of electromagnetic waves by adding a large number of internal electron transfer and transfer channels.
However, in a few electromagnetic wave-absorbing studies on TMDs, the high density and high necessary loading have prevented TMDs from becoming more effective wave-absorbing materials. For example, huang et al [ ACS Nano 2022, 16, 7861-7879]High quality Fe is synthesized 3 GeTe 2 The crystal, whose minimum Reflection Loss (RL) value is-34.7 dB, and whose thickness is required to be 5.5 mm, has a load factor as high as 70 wt%. Therefore, there is an urgent need to optimize the TMDs-based wave absorbing material to meet the requirements of "thin, light, wide, strong" and thus obtain better absorption effect. As described above, the hetero-interface engineering is considered as one of the most promising strategies for pursuing high-performance microwave absorbing materials. Specifically, the heterogeneous interface design inherits unique electromagnetic characteristics of the element, such as dielectric and magnetic properties, optimizes impedance matching and maximizes energy efficiency. In addition, it brings about a range of physicochemical properties including band alignment, space charge, electron transport, lattice defects, lattice strain and pinning effects, which have fundamental effects on dipole polarization, conduction loss and magnetic response, thus contributing to the improvement of the wave absorbing performance.
Disclosure of Invention
In view of the followingThe embodiment of the invention provides an electromagnetic wave absorbing material, and a preparation method and application thereof. Preparation of Cr with heterostructure by using simple and efficient one-step chemical vapor deposition technology 5 Te 8 Expanded graphite (ECT, cr) 5 Te 8 @ Expanded Graphite) wave-absorbing material. Heterostructures give ECT superior wave absorbing properties at lower loadings and thinner thicknesses. The electromagnetic wave absorbing material provided by the invention has the advantages of simple and efficient preparation method and low production cost, and the prepared material has better electromagnetic wave absorbing capacity and radar scattering sectional area (RCS, radar Cross Section) reducing capacity and can effectively dissipate electromagnetic waves.
In order to achieve the above effects, the preparation method of the electromagnetic wave-absorbing material provided by the invention comprises the following specific steps: s1: placing a quartz boat filled with Te blocks at the upstream of a hot zone of a tube furnace; s2: cr is added to 2 O 3 Uniformly mixing the powder and the expandable graphite powder, spreading the mixture in another quartz boat in a thin way, placing the mixture in the central position of a hot zone of a tube furnace, simultaneously carrying out heating treatment on the quartz boat in the step S1 and the other quartz boat in the step S2, and preparing a required material by utilizing a chemical vapor deposition technology; s3: naturally cooling the material prepared in S2 to obtain Cr 5 Te 8 An expanded graphite wave-absorbing material.
Alternatively, cr as described in S2 2 O 3 Powder and expandable graphite powder according to 1:1/10-1:10 mass ratio.
Alternatively, the diameter of the quartz tube in the tube furnace is 1-10 inches.
Optionally, a mixed gas of argon and hydrogen is used as a carrier gas during the whole heating treatment in S2. Optionally, in the mixed gas, the flow rate of argon is 80-120 sccm, and the flow rate of hydrogen is 3-20 sccm.
Optionally, the heating treatment in S2 specifically includes: heating from room temperature for 50 deg.C for min -1 Until the temperature is increased to 680-730 ℃ and maintained at the growth temperature for 2-6 min.
Alternatively, the reaction chamber is purged with high purity argon for 5 minutes prior to the heat treatment described in S2.
Optionally, the flow rate of the high-purity argon is 500 sccm.
In another aspect of the present invention, there is provided Cr prepared by the above preparation method 5 Te 8 An expanded graphite wave-absorbing material.
In another aspect of the invention, a Cr 5 Te 8 The application of the @ expanded graphite wave-absorbing material in the field of electromagnetic protection.
The invention has the beneficial effects that:
(1) Two-dimensional Cr 5 Te 8 Atomic spin magnetism of nano-sheet and lightweight porous conductive expanded graphite construct Cr with magnetoelectric synergy 5 Te 8 Low loading wave absorbing material of expanded graphite.
（2）Cr 5 Te 8 Intimate contact with the expanded graphite may trigger the redistribution of interfacial charges, thereby producing a secondary Cr 5 Te 8 The built-in electric field and the Schottky barrier to the expanded graphite are beneficial to the dense polarization of the interface and the electromagnetic energy consumption.
Thus, cr 5 Te 8 The @ expanded graphite wave-absorbing material has potential application prospect in the field of electromagnetic protection.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure and method steps particularly pointed out in the written description and claims hereof as well as the appended drawings.
It will be appreciated by those skilled in the art that the objects and advantages that can be achieved with the present invention are not limited to the above-described specific ones, and that the above and other objects that can be achieved with the present invention will be more clearly understood from the following detailed description.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate and together with the description serve to explain the invention.
FIG. 1 is a drawing of Cr in example 1 of the present invention 5 Te 8 SEM image of @ expanded graphite wave-absorbing material;
FIG. 2 is a diagram of example 2 Cr of the present invention 5 Te 8 Cr in @ expanded graphite wave-absorbing material 5 Te 8 XPS spectra of (a);
FIG. 3 is a graph showing the results of the 3D reflection loss of comparative example 1 at a loading of 10% according to the present invention;
FIG. 4 is a graph of the 3D reflection loss results of comparative example 2 at a loading of 10% according to the present invention;
FIG. 5 is a graph showing Cr content of example 3 at a loading of 10% according to the present invention 5 Te 8 3D reflection loss result diagram of the @ expanded graphite wave-absorbing material in the frequency range of 2-18 GHz;
FIG. 6 is a graph showing Cr content of example 3 at a loading of 10% according to the present invention 5 Te 8 2D reflection loss result diagram of the @ expanded graphite wave-absorbing material in the frequency range of 2-18 GHz;
FIG. 7 is a graph showing Cr content of example 6 at a loading of 10% according to the present invention 5 Te 8 3D reflection loss result diagram of the @ expanded graphite wave-absorbing material in the frequency range of 2-18 GHz;
FIG. 8 is a graph showing the Cr content of example 6 at a loading of 10% according to the present invention 5 Te 8 2D reflection loss result diagram of the @ expanded graphite wave-absorbing material in the frequency range of 2-18 GHz;
FIG. 9 is a graph of the simulation results of the 3D radar signal of comparative example 1 of the present invention;
fig. 10 is a diagram of simulation results of 3D radar scattering signals according to embodiment 2 of the present invention;
fig. 11 is a graph showing the simulation result of the 3D radar scattering signal according to comparative example 2 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments and the accompanying drawings, for the purpose of making the objects, technical solutions and advantages of the present invention more apparent, and the illustrative embodiments of the present invention and the descriptions thereof are used for explaining the present invention, but not limiting the present invention. It should be noted here that, in order to avoid obscuring the present invention due to unnecessary details, only structures and/or processing steps closely related to the solution according to the present invention are shown in the drawings, while other details not greatly related to the present invention are omitted.
It should be emphasized that the term "comprises/comprising" when used herein is taken to specify the presence of stated features, elements, steps or components, but does not preclude the presence or addition of one or more other features, elements, steps or components.
The embodiment of the invention provides an electromagnetic wave-absorbing material, and a preparation method and application thereof. Thanks to Cr 5 Te 8 And strong interfacial polarization relaxation due to heterogeneous interface of expanded graphite, cr 5 Te 8 The magnetic loss caused by strong atomic spin and the synergistic effect among rich interlayer scattering optimize the impedance matching of the ECT wave-absorbing material, so that the ECTs wave-absorbing material has excellent electromagnetic wave-absorbing performance.
Specifically, the preparation method of the electromagnetic wave-absorbing material provided by the invention comprises the following specific steps: s1: placing a quartz boat filled with Te blocks at the upstream of a hot zone of a tube furnace; s2: cr is added to 2 O 3 Uniformly mixing the powder and the expandable graphite powder, thinly paving the mixture in another quartz boat and placing the mixture in the central position of a hot zone of a tubular furnace, simultaneously carrying out heating treatment on the quartz boat in S1 and the other quartz boat in S2, and preparing a required material by utilizing a chemical vapor deposition technology; s3: naturally cooling the material prepared in S2 to obtain Cr 5 Te 8 An expanded graphite wave-absorbing material.
Alternatively, cr in S2 2 O 3 Powder and expandable graphite powder according to 1:1/10-1:10 mass ratio.
Alternatively, the diameter of the quartz tube in the tube furnace is 1-10 inches.
Optionally, the mixed gas of argon and hydrogen is used as carrier gas in the whole heating treatment process in the step S2.
Optionally, in the mixed gas, the flow rate of argon is 80-120 sccm, and the flow rate of hydrogen is 3-20 sccm.
Optionally, the heating treatment in S2 includes: heating from room temperature for 50 deg.C for min -1 Is a straight lineHeating to 680-730 deg.C, and maintaining at growth temperature for 2-6 min.
Alternatively, the reaction chamber is purged with high purity argon for 5 minutes before heating in S2.
Alternatively, the flow rate of high purity argon is 500 sccm.
In another aspect of the present invention, there is provided Cr prepared by the above preparation method 5 Te 8 An expanded graphite wave-absorbing material.
In another aspect of the invention, a Cr 5 Te 8 The application of the @ expanded graphite wave-absorbing material in the field of electromagnetic protection.
The invention is further illustrated by the following examples, which are intended to be illustrative only and not limiting in any way.
Example 1
A quartz boat filled with Te blocks was placed upstream of the tube furnace hot zone, which was at a temperature of about 500 ℃. Taking 1 part by mass of Cr 2 O 3 Powder and 1/10 Cr 2 O 3 The primary expandable graphite powder is uniformly mixed in parts by mass, and is thinly spread in a quartz boat, and then the quartz boat is placed in a quartz tube with a diameter of one inch and is placed in the center of a hot zone of a tube furnace. Purging the reaction chamber with high purity argon (Ar, 500 sccm) for 5 min before heating, and heating with Ar and H 2 Is used as carrier gas, ar flow is 100 sccm, H 2 The flow rate was 10 sccm. The growth temperature is set to 720 ℃, and the temperature rising rate is set to 50 ℃ for min -1 And maintained for 3 min. After the reaction is completed, naturally cooling to obtain Cr 5 Te 8 An SEM picture of the @ expanded graphite wave-absorbing material is shown in fig. 1.
Example 2
A quartz boat filled with Te blocks was placed upstream of the tube furnace hot zone, which was at a temperature of about 500 ℃. Taking 1 part by mass of Cr 2 O 3 Powder and 10 times Cr 2 O 3 Uniformly mixing primary expandable graphite powder in parts by mass, thin-laying the mixture in another quartz boat, and placing the other quartz boat in a quartz tube with a diameter of one inch and placing the quartz boat in parallelAt the center of the hot zone of the tube furnace. Purging the reaction chamber with high purity argon (Ar, 500 sccm) for 5 min before heating, and heating with Ar and H 2 Is used as carrier gas, ar flow is 80 sccm, H 2 The flow rate was 20 sccm. The growth temperature is set to 680 ℃, and the temperature rising rate is set to 50 ℃ for min -1 And maintained for 6 min. After the reaction is completed, naturally cooling to obtain Cr 5 Te 8 The XPS spectrum of the expanded graphite wave-absorbing material is shown in figure 2, and the XPS spectrum is matched with pure Cr 5 Te 8 In contrast, the peaks of both Cr and Te for ECT are shifted to higher binding energies by about 0.2-0.3. 0.3 eV, confirming that electrons are driven from Cr 5 Te 8 Transfer to the expanded graphite side illustrates the successful construction of the heterojunction. The 3D radar reflected signal intensity graph is shown in fig. 10.
Example 3
A quartz boat filled with Te blocks was placed upstream of the tube furnace hot zone, which was at a temperature of about 500 ℃. Taking 1 part by mass of Cr 2 O 3 The powder was mixed with the same mass portion of primary expandable graphite powder and thinly laid in another quartz boat, which was then placed in a quartz tube having a diameter of one inch and placed in the center of the hot zone of the tube furnace. Purging the reaction chamber with high purity argon (Ar, 500 sccm) for 5 min before heating, and heating with Ar and H 2 Is used as carrier gas, ar flow is 100 sccm, H 2 The flow rate was 8 sccm. The growth temperature is set to 730 ℃, and the temperature rising rate is set to 50 ℃ for min -1 And maintained for 5 min. After the reaction is completed, naturally cooling to obtain Cr 5 Te 8 The wave absorbing performance of the @ expanded graphite wave absorbing material is shown in figures 5 and 6.
Example 4
A quartz boat filled with Te blocks was placed upstream of the tube furnace hot zone, which was at a temperature of about 500 ℃. Taking 1 part by mass of Cr 2 O 3 Powder and 4 times Cr 2 O 3 The primary expandable graphite powder was uniformly mixed in parts by mass and thinly laid in another quartz boat, and then the other quartz boat was placed in a quartz tube having a diameter of one inch and placed in the center of the hot zone of the tube furnace. Purging the reaction chamber with high purity argon (Ar, 500 sccm) for 5 min before heating, and heating at Ar and H 2 Is used as carrier gas, ar flow is 120 sccm, H 2 The flow rate was 3 sccm. The growth temperature is set to 700 ℃, and the temperature rising rate is set to 50 ℃ for min -1 And maintained for 2 min. After the reaction is completed, naturally cooling to obtain Cr 5 Te 8 An expanded graphite wave-absorbing material.
Example 5
A quartz boat filled with Te blocks was placed upstream of the tube furnace hot zone, which was at a temperature of about 500 ℃. Taking 1 part by mass of Cr 2 O 3 Powder and 1/3 Cr 2 O 3 The primary expandable graphite powder was uniformly mixed in parts by mass and thinly laid in another quartz boat, and then the other quartz boat was placed in a quartz tube having a diameter of one inch and placed in the center of the hot zone of the tube furnace. Purging the reaction chamber with high purity argon (Ar, 500 sccm) for 5 min before heating, and heating with Ar and H 2 Is used as carrier gas, ar flow is 110 sccm, H 2 The flow rate was 5 sccm. The growth temperature is set to 710 ℃, and the temperature rising rate is set to 50 ℃ for min -1 And maintained for 4 min. After the reaction is completed, naturally cooling to obtain Cr 5 Te 8 An expanded graphite wave-absorbing material.
Example 6
A quartz boat filled with Te blocks was placed upstream of the tube furnace hot zone, which was at a temperature of about 500 ℃. Taking 1 part by mass of Cr 2 O 3 Powder and 2 times Cr 2 O 3 The primary expandable graphite powder was uniformly mixed in parts by mass and thinly laid in another quartz boat, and then the other quartz boat was placed in a quartz tube having a diameter of one inch and placed in the center of the hot zone of the tube furnace. Purging the reaction chamber with high purity argon (Ar, 500 sccm) for 5 min before heating, and heating with Ar and H 2 Is used as carrier gas, ar flow is 95 sccm, H 2 The flow rate was 12 sccm. The growth temperature is set to 690 ℃, and the temperature rising rate is 50 ℃ for min -1 And maintained for 5 min. After the reaction is completed, naturally cooling to obtain Cr 5 Te 8 The wave absorbing performance of the @ expanded graphite wave absorbing material is shown in figures 7 and 8.
Example 7
Placing quartz boat filled with Te block in tubeUpstream of the furnace hot zone, the hot zone temperature was about 500 ℃. Taking 1 part by mass of Cr 2 O 3 Powder and 3 times Cr 2 O 3 The primary expandable graphite powder was uniformly mixed in parts by mass and thinly laid in another quartz boat, and then the other quartz boat was placed in a quartz tube having a diameter of one inch and placed in the center of the hot zone of the tube furnace. Purging the reaction chamber with high purity argon (Ar, 500 sccm) for 5 min before heating, and heating with Ar and H 2 The mixed gas of (2) is used as carrier gas, ar flow is 80-120 sccm, H 2 The flow rate is 3-20 sccm. The growth temperature is 680-730 ℃, and the temperature rising rate is 50 ℃ for min -1 And maintained for 2-6 min. After the reaction is completed, naturally cooling to obtain Cr 5 Te 8 An expanded graphite wave-absorbing material.
Comparative example 1
A quartz boat filled with Te blocks was placed upstream of the tube furnace hot zone, which was at a temperature of about 500 ℃. Taking 1 part by mass of Cr 2 O 3 The powder was laid flat in another quartz boat, which was then placed in a quartz tube having a diameter of one inch and placed in the center of the hot zone of the tube furnace. Purging the reaction chamber with high purity argon (Ar, 500 sccm) for 5 min before heating, and heating with Ar and H 2 Is used as carrier gas, ar flow is 100 sccm, H 2 The flow rate was 10 sccm. Cr (Cr) 5 Te 8 The growth temperature of (C) is 720 ℃, and the temperature rising rate is 50 ℃ for min -1 And maintained for 3 min. After the reaction is completed, naturally cooling to obtain Cr 5 Te 8 The wave absorbing performance is shown in fig. 3, and the reflected signal intensity diagram of the 3D radar is shown in fig. 9.
Comparative example 2
1 part by mass of primary expandable graphite powder was laid flat in a quartz boat, and then the quartz boat was placed in a quartz tube having a diameter of one inch and placed in the center of the hot zone of a tube furnace. Purging the reaction chamber with high purity argon (Ar, 500 sccm) for 5 min before heating, and heating with Ar and H 2 Is used as carrier gas, ar flow is 100 sccm, H 2 The flow rate was 10 sccm. The reaction temperature is set to 720 ℃, and the temperature rising rate is set to 50 ℃ for min -1 And maintained for 3 min. After the reaction is completed, naturally cooling to obtainThe wave absorbing performance of the expanded graphite is shown in fig. 4, and the 3D radar reflection signal intensity diagram is shown in fig. 11.
TABLE 1 Cr at different reaction times and reactant mass ratios 5 Te 8 Partial performance parameters of @ expanded graphite wave-absorbing material
The larger the RL value, the better the wave absorbing effect. When RL is less than-10 dB, 90% of the incident electromagnetic waves can be absorbed and converted to thermal energy. The frequency range with RL values less than-10 dB is the effective absorption bandwidth. As shown in FIGS. 5 and 7, cr produced by the present invention 5 Te 8 The @ expanded graphite wave-absorbing material has excellent wave-absorbing performance, and when the load capacity of the material with paraffin is 10 wt percent and the thickness is 1.4 mm, the maximum reflection loss value can reach-57.6 dB; as shown in fig. 6 and 8, the Effective Absorption Bandwidth (EAB) can reach 4.6 GHz at a thickness of 1.6 mm. Compared with the comparative example, cr 5 Te 8 The @ expanded graphite wave-absorbing material has more outstanding wave-absorbing performance, and the material benefits from the fact that a heterostructure induces a strong interfacial polarization relaxation mechanism to provide good conditions for optimizing impedance matching. As shown by the RCS simulation results of FIGS. 9-11, cr 5 Te 8 The radar reflection signal intensity of the @ expanded graphite is the lowest, which indicates the excellent radar wave scattering capability.
Electromagnetic loss capacity and radar stealth capacity of the ECT under near-actual conditions are verified through radar reflection sectional area simulation.
In addition, cr prepared by the invention 5 Te 8 The @ expanded graphite wave-absorbing material has the characteristics of low load and excellent electromagnetic wave-absorbing performance, and the preparation method is simple, easy to operate and low in production cost, and meets the electromagnetic protection requirement of electronic equipment.
While the foregoing is directed to embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (10)
1. Cr (chromium) 5 Te 8 The preparation method of the electromagnetic wave-absorbing material of the expanded graphite is characterized by comprising the following specific steps:
s1: placing a quartz boat filled with Te blocks at the upstream of a hot zone of a tube furnace;
s2: cr is added to 2 O 3 Uniformly mixing the powder and the expandable graphite powder, spreading the mixture in another quartz boat in a thin way, placing the mixture in the central position of a hot zone of a tube furnace, simultaneously carrying out heating treatment on the quartz boat in the step S1 and the other quartz boat in the step S2, and preparing a required material by utilizing a chemical vapor deposition technology;
s3: naturally cooling the material prepared in S2 to obtain Cr 5 Te 8 An expanded graphite wave-absorbing material.
2. The method of manufacturing according to claim 1, characterized in that: cr as described in S2 2 O 3 Powder and expandable graphite powder according to 1:1/10-1:10 mass ratio.
3. The method of manufacturing according to claim 1, characterized in that: the diameter of the quartz tube in the tube furnace is 1-10 inches.
4. A method of preparation according to claim 3, characterized in that: and S2, taking a mixed gas of argon and hydrogen as a carrier gas in the whole heating treatment process.
5. The method of manufacturing according to claim 4, wherein: in the mixed gas, the flow rate of argon is 80-120 sccm, and the flow rate of hydrogen is 3-20 sccm.
6. The method according to claim 4, wherein the heating treatment in S2 specifically comprises: heating from room temperature to 50deg.C min -1 Until the temperature is increased to 680-730 ℃ and maintained at the growth temperature for 2-6 min.
7. The method of manufacturing according to claim 1, characterized in that: before the heating treatment in S2, the reaction chamber is purged for 5 minutes by high-purity argon gas so as to remove oxygen in the tubular furnace chamber and facilitate two-dimensional Cr 5 Te 8 Is a growth of (a).
8. The method of manufacturing according to claim 7, wherein: the flow rate of the high-purity argon is 500 sccm.
9. Cr prepared by the preparation method according to any one of claims 1-8 5 Te 8 An expanded graphite wave-absorbing material.
10. Cr according to claim 9 5 Te 8 The application of the @ expanded graphite wave-absorbing material in the field of electromagnetic protection.
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